CN104119913B - A kind of near ultraviolet excitated phosphoric acid salt white fluorescent powder and preparation method thereof - Google Patents
A kind of near ultraviolet excitated phosphoric acid salt white fluorescent powder and preparation method thereof Download PDFInfo
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- CN104119913B CN104119913B CN201410382922.3A CN201410382922A CN104119913B CN 104119913 B CN104119913 B CN 104119913B CN 201410382922 A CN201410382922 A CN 201410382922A CN 104119913 B CN104119913 B CN 104119913B
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- phosphoric acid
- acid salt
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- fluorescent powder
- white fluorescent
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- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention discloses a kind of near ultraviolet excitated phosphoric acid salt white fluorescent powder and preparation method thereof, combination matching general formula is La
0.98-xpO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ x, x is Eu
3+molecular fraction in this compound, wherein 0 < x≤0.1.Its preparation method is by compound Homogeneous phase mixing corresponding to La, Ce, Li, Eu, then adds phosphoric acid salt, grinds after mixing, and insulation obtains presoma; Presoma described in roasting obtains near ultraviolet excitated phosphoric acid salt white fluorescent powder.The commercial near-ultraviolet ray that phosphoric acid salt white fluorescent powder of the present invention can be 370 ~ 410nm by wavelength excites; have good market outlook, and the productive rate that the method obtains is more than 99%, roasting process does not need the protection of reducing atmosphere; easy to control, technique is simple.
Description
Technical field
The invention belongs to fluorescent material preparation field, particularly relate to a kind of near ultraviolet excitated phosphoric acid salt white fluorescent powder and preparation method thereof, and this fluorescent material is for mixing cerium, lithium, europium lanthanum orthophosphate white fluorescent powder.
Background technology
White light emitting diode (LEDs) has the advantages such as luminous efficiency is high, energy-conservation, the life-span is long, energy consumption is low, environmental protection.Therefore, LEDs is regarded as the Sony ericsson mobile comm ab of a new generation.The focus of current research mainly concentrates on the research and development of novel single-matrix white light-emitting fluorescent material, to develop the fluorescent material that can improve white LEDs luminescent properties.
Such as, the typical single-matrix white luminescent phosphor developed has the Ca of phosphoric acid salt
9lu(PO
4)
7: Eu
2+, Mn
2+and the Ca of silicophosphate class
5la
5(SiO
4)
3(PO
4)
3o
2: Ce
3+, Mn
2+; But the wavelength ratio of these fluorescent material exciting light used is shorter, do not mate with the wavelength (370 ~ 410nm) of commercial near ultraviolet chip.Therefore, synthesis can be excited by ultraviolet chip (370 ~ 410nm), the phosphoric acid salt list substrate fluorescent powder that has of High Efficiency Luminescence advances the business-like important behave of single-matrix white luminescent phosphor.
The preparation method being mixed with the single-matrix white luminescent phosphor of two kinds of light emitting ionics has many sections of bibliographical informations, but these are reported or are Eu
2+, Mn
2+the combination of ion, or be exactly Ce
3+, Mn
2+the combination of ion, and exciting light used does not mate with the wavelength (370 ~ 410nm) of commercial near ultraviolet chip, and namely the ripple of exciting light used is less than 370nm.Therefore, still lack so far can the single-matrix white fluorescent material that excites by about 390nm light.
Summary of the invention
The object of this invention is to provide a kind of white fluorescent powder, to solve wavelength (370 ~ 410nm) the unmatched deficiency of existing fluorescent material and commercial near ultraviolet chip.
Technical scheme of the present invention:
A near ultraviolet excitated phosphoric acid salt white fluorescent powder, is characterized in that: its combination matching general formula is La
0.98-xpO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ x, x is Eu
3+molecular fraction in this compound, wherein 0 < x≤0.1.
Further, described x=0.01,0.02,0.03,0.04,0.05,0.06,0.07,0.08,0.09 or 0.1.
Further, in raw material, containing La
3+compound be selected from a kind of in lanthanum trioxide, lanthanum oxalate, Phosbloc, lanthanum nitrate or several combination in compatible situation.
Further, in raw material, containing Ce
3+compound be selected from a kind of in cerium oxide, Sedemesis, cerous carbonate, cerous nitrate or several combination in compatible situation.
Further, in raw material, containing Li
+compound be selected from a kind of in lithium chloride, lithium nitrate, Quilonum Retard, hydrogen lithium hydride, Lithium Oxide 98min or several combination in compatible situation.
Further, in raw material, containing Eu
3+compound be selected from a kind of in europium sesquioxide, oxalic acid europium, europium carbonate, europium nitrate or several combination in compatible situation.
Further, in raw material, containing PO
4 3+compound be selected from triammonium phosphate, ammonium hydrogen phosphate, primary ammonium phosphate a kind of or several combination in compatible situation, phosphoric acid salt contains crystal water.
Another technical scheme of the present invention:
Prepare the method for near ultraviolet excitated phosphoric acid salt white fluorescent powder: by compound Homogeneous phase mixing corresponding to La, Ce, Li, Eu, then add phosphoric acid salt, grind after mixing, insulation obtains presoma; Presoma described in roasting obtains near ultraviolet excitated phosphoric acid salt white fluorescent powder.
Further, described milling time is 10-120min.
Further, insulation obtains the condition of presoma is 120 DEG C of insulations 3 hours.
Further, when containing nitrate in raw material, described presoma, first 300 DEG C of roastings 3 hours, is then warmed up to 780 DEG C and continues roastings 3 hours.Low-temperature bake in first paragraph 300 DEG C, mainly allows by product ammonium nitrate smoothly, without explosion hazard be decomposed into harmless aqueous vapor and nitrogen; Second segment 780 DEG C of high-temperature roastings, mainly allow reactant form the product of crystallized form.
Further, when containing muriate in raw material, described presoma, first 300 DEG C of roastings 3 hours, is then warmed up to 780 DEG C and continues roastings 3 hours.Low-temperature bake in first paragraph 300 DEG C, mainly allows by-product ammonium chloride divide and takes off, in order to avoid its roasting and other substance reaction under follow-up high temperature generate impurity; Second segment 780 DEG C of high-temperature roastings, mainly allow reactant form the product of crystallized form.
Advantage of the present invention:
Compared with prior art, productive rate, more than 99%, has the protection that roasting process does not need reducing atmosphere to method of the present invention, easy to control, and technique is simple, raw material sources are wide, is easy to the advantages such as suitability for industrialized production;
Characteristic of the present invention is that excitation wavelength used is 394nm, and the wavelength of this exciting light and the wavelength (370 ~ 410nm) of commercial near ultraviolet chip match, can be excited by commercial near ultraviolet chip and obtain white light mix cerium, lithium, europium lanthanum orthophosphate (La
0.98-xpO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ x) single-matrix white luminescent phosphor.
Accompanying drawing explanation
When Fig. 1 is x=0.04 in the embodiment of the present invention 4, the X-ray diffraction of products therefrom analyzes collection of illustrative plates (XRD).
The excitation spectrum (PLE) of products therefrom when Fig. 2 is x=0.04 in the embodiment of the present invention 4.
The emmission spectrum (PL) of products therefrom when Fig. 3 is x=0.04 in the embodiment of the present invention 4.
The chromaticity coordinates figure (x=0.38, y=0.34) of products therefrom when Fig. 4 is x=0.04 in the embodiment of the present invention 4.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can do various amendment or change to the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Preparation [La
0.97pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.01], x=0.01.
Get lanthanum trioxide La
2o
3powder 7.275mol and 2370.5g, cerous nitrate Ce(NO
3)
36H
2o powder 0.15 mol, i.e. 65.1g, europium nitrate Eu(NO
3)
36H
2o powder 0.15 mol, i.e. 66.9g, Quilonum Retard Li
2cO
3powder 0.225mol, i.e. 16.63g, primary ammonium phosphate (NH
4) H
2pO
4powder 15.0 mol, i.e. 1725.4g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium nitrate powder and lithium carbonate powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add primary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 10 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 3h, be again warmed up to 780 DEG C and continue roasting 3h, obtain La
0.97pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.01, yield is 99.6%(take phosphate radical as benchmark).
Embodiment 2
Preparation [La
0.96pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.02], x=0.02.
Get lanthanum trioxide La
2o
3powder 7.2 mol, i.e. 2346.0g, cerous nitrate Ce(NO
3)
36H
2o powder 0.15 mol and 65.1g, europium sesquioxide Eu
2o
3powder 0.15 mol, i.e. 43.3g, Quilonum Retard Li
2cO
3powder 0.225mol, i.e. 16.63g, primary ammonium phosphate (NH
4) H
2pO
4powder 15.0 mol, i.e. 1725.4g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium sesquioxide powder and lithium carbonate powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add primary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 30 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 4h, be again warmed up to 780 DEG C and continue roasting 3h, obtain La
0.96pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.02, yield is 99.1%(take phosphate radical as benchmark).
Embodiment 3
Preparation [La
0.95pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.03], x=0.03.
Get lanthanum nitrate La(NO
3)
36H
2o powder 14.25mol, i.e. 6170.4g, cerous nitrate Ce(NO
3)
36H
2o powder 0.15mol, i.e. 65.1g, europium sesquioxide Eu
2o
3powder 0.225mol, i.e. 64.9g, Quilonum Retard Li
2cO
3powder 0.225mol, i.e. 16.63g, primary ammonium phosphate (NH
4) H
2pO
4powder 15.0 mol, i.e. 1725.4g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium sesquioxide powder and lithium carbonate powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add primary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 50 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 3h, be again warmed up to 780 DEG C and continue roasting 5h, obtain La
0.95pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.03, yield is 99.4%(take phosphate radical as benchmark).
Embodiment 4
Preparation [La
0.94pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.04], x=0.04.
Get lanthanum trioxide La
2o
3powder 7.05mol, 2297.2g, cerous nitrate Ce(NO
3)
36H
2o powder 0.15mol, i.e. 65.1g, europium nitrate Eu(NO
3)
36H
2o powder 0.60mol, i.e. 267.6g, lithium hydroxide LiOH powder 0.45mol, i.e. 10.78g, primary ammonium phosphate (NH
4) H
2pO
4powder 15.0mol, i.e. 1725.4g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium nitrate powder and lithium hydroxide powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add primary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 70 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 5h, be again warmed up to 780 DEG C and continue roasting 4h, obtain La
0.94pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.04, yield is 99.7%(take phosphate radical as benchmark).
Embodiment 5
Preparation [La
0.93pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.05], x=0.05.
Get lanthanum trioxide La
2o
3powder 6.975mol, i.e. 2272.7g, cerous nitrate Ce(NO
3)
36H
2o powder 0.15mol, i.e. 65.1g, europium nitrate Eu(NO
3)
36H
2o powder 0.75 mol, i.e. 334.6g, Quilonum Retard Li
2cO
3powder 0.225mol, i.e. 16.63g, Secondary ammonium phosphate (NH
4)
2hPO
4powder 15.0 mol, i.e. 1980.8g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium nitrate powder and lithium hydroxide powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add Secondary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 90 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 5h, be again warmed up to 780 DEG C and continue roasting 3h, obtain La
0.93pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.05, yield is 99.3%(take phosphate radical as benchmark).
Embodiment 6
Preparation [La
0.92pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.06], x=0.06.
Get lanthanum trioxide La2O3 powder 6.9mol, i.e. 2248.3g, cerous nitrate Ce(NO
3) 36H
2o powder 0.15 mol, i.e. 65.1g, europium nitrate Eu(NO
3) 36H
2o powder 0.90 mol, i.e. 401.5g, lithium hydroxide LiOH powder 0.45mol, i.e. 10.78g, triammonium phosphate (NH
4)
3pO
43H
2o powder 15.0 mol, i.e. 3047.0g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium nitrate powder and lithium hydroxide powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add Secondary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 1200 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 5h, be again warmed up to 780 DEG C and continue roasting 3h, obtain La
0.92pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.06powder crystal, yield is 99.3%(take phosphate radical as benchmark).
Embodiment 7
Preparation [La
0.97pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.01], x=0.01.
Get lanthanum trioxide La
2o
3powder 7.275mol and 2370.5g, Cerium II Chloride CeCl
37H
2o powder 0.15 mol, i.e. 55.89g, Europium trichloride EuCl
36H
2o powder 0.15 mol, i.e. 54.96g, Quilonum Retard Li
2cO
3powder 0.225mol, i.e. 16.63g, primary ammonium phosphate (NH
4) H
2pO
4powder 15.0 mol, i.e. 1725.4g.
In an enamelled vessel, add lanthanum oxide powder, cerous nitrate powder, europium nitrate powder and lithium carbonate powder mixes for subsequent use, then at room temperature, normal pressure, in above-mentioned mixed powder, add primary ammonium phosphate powder under whipped state, add to mix in rear immigration grinding plant and fully grind 10 min.First, in baking oven, at 120 DEG C, insulation leaves standstill 3h, its inferior in muffle furnace at 300 DEG C roasting 4h, be again warmed up to 780 DEG C and continue roasting 3h, obtain La
0.97pO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ 0.01, yield is 99.5%(take phosphate radical as benchmark).
Product in Example 4, carries out XRD analysis, fluorescent spectroscopy, and result shows that products therefrom mixes cerium, lithium, europium lanthanum orthophosphate crystal, because structure is identical with lanthanum orthophosphate.
The near ultraviolet excitated white fluorescent material prepared excites effectively to launch and obtain white light after the emission peak integer combinations in 420-750nm region under 394 nm, as shown in Figures 2 and 3, its CIE chromaticity coordinates at white light field (x=0.38, y=0.34), as shown in Figure 4.
By the inspiration of above-described embodiment, those of ordinary skill in the art can obtain different Eu by aforesaid method
3+the different embodiments of molecular fraction, namely can obtain the different embodiments in 0 < x≤0.1 scope, and those of ordinary skill in the art can obtain identical or close expected technique effect.
Claims (8)
1. a near ultraviolet excitated phosphoric acid salt white fluorescent powder, is characterized in that: its combination matching general formula is La
0.98-xpO
4: Ce
3+ 0.01, Li
+ 0.03, Eu
3+ x, x is Eu
3+molecular fraction in this compound, wherein 0 < x≤0.1.
2. phosphoric acid salt white fluorescent powder near ultraviolet excitated as claimed in claim 1, is characterized in that: described x=0.01,0.02,0.03,0.04,0.05,0.06,0.07,0.08,0.09 or 0.1.
3. the method for the phosphoric acid salt white fluorescent powder that preparation is near ultraviolet excitated as claimed in claim 1 or 2, it is characterized in that: by compound Homogeneous phase mixing corresponding to La, Ce, Li, Eu, then add phosphoric acid salt, grind after mixing, insulation obtains presoma; Presoma described in roasting obtains near ultraviolet excitated phosphoric acid salt white fluorescent powder.
4. phosphoric acid salt white fluorescent powder near ultraviolet excitated as claimed in claim 3, is characterized in that:
The compound that La is corresponding is selected from a kind of in lanthanum trioxide, lanthanum oxalate, Phosbloc, lanthanum nitrate or several combination in compatible situation;
The compound that Ce is corresponding is selected from a kind of in cerium oxide, Sedemesis, cerous carbonate, cerous nitrate or several combination in compatible situation;
The compound that Li is corresponding is selected from a kind of in lithium chloride, lithium nitrate, Quilonum Retard, hydrogen lithium hydride, Lithium Oxide 98min or several combination in compatible situation;
The compound that Eu is corresponding is selected from a kind of in europium sesquioxide, oxalic acid europium, europium carbonate, europium nitrate or several combination in compatible situation;
Phosphoric acid salt is selected from triammonium phosphate, ammonium hydrogen phosphate, primary ammonium phosphate a kind of or several combination in compatible situation.
5. method as claimed in claim 3, is characterized in that: the time of described grinding step is 10-120min.
6. method as claimed in claim 3, is characterized in that: the condition that insulation obtains presoma is 120 DEG C of insulation 3-5 hour.
7. method as claimed in claim 3, is characterized in that: when containing nitrate in raw material, and described presoma, first at 300 DEG C of roasting 3-5 hour, is then warmed up to 780 DEG C and continues roasting 3-5 hour.
8. method as claimed in claim 3, is characterized in that: when containing muriate in raw material, and described presoma, first at 300 DEG C of roasting 3-5 hour, is then warmed up to 780 DEG C and continues roasting 3-5 hour.
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|---|---|---|---|
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